Development and Validation of a Simple and Fast Method for Sulfonamides, Tetracyclines and Macrolides in Honey Using Lc-MS/MS

Abstract

Antibacterial are widely used in veterinary applications for diseases treatment and prophilatic purposes. Inadequate uses of these drugs can lead of undesirable residues in honey for consumption. In Brazil, the legal authorities set a maximum residue limit (MRL) for different compound in honey, ranging from 10 to 20 ng ml-1. The monitoring of antibacterials is a concern, since it constitutes a risk to human health and collaborates with the growth of resistant bacteria. Brazil has the National Residue Control Plan (NRCP) to ensure that the products traded are compliant with the safety and quality criteria required by consumers. The goal of this work was to develop and validate a method suitable to determine sulfonamides, tetracyclines and macrolides in honey, using liquid chromatography tandem mass spectrometry. The main objective was to develop an efficient technique, combining simplicity, speed and low cost, since the method will be employed in routine analysis. Recoveries between 36 to 139% were obtained. Good linearity (r2) above 0.95, considering three different days, for all drugs was achieved in concentrations ranging from 0 to 200% of the MRL. Intraday and inter-day precision with CV% (n=6) lower than 18%, in agreement with specifications were obtained in concentrations ranging from 0.5 to 1.5 MRL, except for erythromycin. Accuracy was between 97 to 108%. Limits of quantitation for macrolides were 2.5 ng g-1and for sulfonamides and tetracyclines were 5 ng g-1. Decision limit (CCα) was evaluated and the results obtained were between 12.9 to 28.1 ng g-1. The detection capability (CCβ) obtained was between 15.8 to 36.3 ng g-1. The proposed method demonstrated to be suitable for this intended purpose and will contribute to antibacterial honey monitoring.

Assessment of various veterinary drug residues in animal originated food products

“…[32]. Ribeiro et al [33] developed and validated a method to determine Sulfa + , Tet + , and macrolides in honey sample, using LC-MS/MS according to Council Directive 657/EC/2002. Recoveries between 36 and 139% were obtained.…”